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31results about How to "Control supersaturation" patented technology

Method for preparing nano catalytic composite materials by utilizing integrating process of ultrasonic-film-anti-solvent method

The invention relates to a method for preparing nano catalytic composite materials by utilizing an integrating process of an ultrasonic-film-anti-solvent method, comprising the following steps of: (1) the ammonium porchlorate saturated solution preparation process: dissolving ammonium porchlorate into a proper solvent to prepare the ammonium porchlorate saturated solution at certain temperature; (2) the dispersing process of a nano catalyst: uniformly dispersing the nano catalyst into an anti-solvent under ultrasonic action; (3) the preparing process: adding the AP (ammonium porchlorate) saturated solution to a nonsolvent through a film tube under certain pressure, wherein after the anti-solvent carries out desolvation on the solvent, the ammonium porchlorate is separated out and covers on the surfaces of uniformly-dispersed nano particles to form the nano catalytic composite materials; (4) filtering and drying processes: firstly carrying out solid-liquid separation on nano composite particles; and (5) the drying process: drying separated materials at 50-150 DEG C to obtain the nano catalytic composite materials. The nano catalytic composite materials prepared by the method have stable structure, uniform nano catalyst dispersion and controllable particle diameter and appearance.
Owner:NANJING NORMAL UNIVERSITY

Surface erosion-resistant composite coating of carbon/carbon composite, preparation method and application thereof

The invention relates to a surface erosion-resistant composite coating of a carbon/carbon composite, which sequentially consists of ZrC0.7/ZrC1.0/ZrC1.0+C form outside to inside. The preparation method of the surface erosion-resistant composite coating comprises the following three steps: the preparation of a basal layer ZrC1.0+C, the preparation of a middle layer ZrC1.0 and the preparation of an outer-coating layer ZrC0.7; and is characterized in that in a chemical vapor deposition furnace at normal pressure, zirconium tetrachloride is used as the zirconium source, Ar gas is used as the carrier gas, C3H6, acetylene and methane are respectively used as the carbon source gasses, Ar is used as the diluent, H2 is used as the reducing gas, and the surface erosion-resistant composite coating is obtained by deposition at the temperature of 1100-1300 DEG C. The invention has the advantages of simple process method, convenient operation, single heat, stepwise deposition preparation of the composite coating with gradient-changed carbon contents, firm combination between the coating and the basal body, no penetration crack and interlayer crack, and good coating erosion resistance and thermal shock resistance, can realize the industrialized production, and is applicable to the preparation of the erosion-resistant composite coating of the carbon/carbon composite by the chemical gas-phase permeation or the liquid-phase impregnation process.
Owner:CENT SOUTH UNIV

Preparation method of fibrous alkali magnesium sulfate whisker

The invention relates to the preparation field of chemical industrial materials, and particularly relates to a preparation method of a fibrous alkali magnesium sulfate whisker. The preparation method of the fibrous alkali magnesium sulfate whisker comprises the following steps: (1) preparing a magnesium sulfate solution by using MgSO4.7H2O, stirring and adding NaOH granular caustic soda, aging for 2-24 hours at the temperature of 25 to 100 DEG C to obtain a slurry; (2) transferring the slurry obtained in the step (1) into a hydrothermal reactor, wherein the filling degree is 50-80 percent, adding 0.5-5 percent of seed crystal according to the mass of the NaOH granular caustic soda, uniformly stirring, and reacting the slurry for 2-12 hours at the temperature of 130-180 DEG C; (3) cooling after finishing the reaction of the step (2), filtering, washing and drying a obtained white turbid liquid to obtain the fibrous alkali magnesium sulfate whisker. According to the preparation method, the seed crystal is added into the reaction slurry, alkali magnesium sulfate is easily subjected to nucleus formation growth, and the preparation concentration of the reaction slurry can be relatively high; the whisker nucleation time is reduced, and the whisker growth time also can be shortened.
Owner:QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI

Low-temperature method for manufacturing nano-MgO crystal whisker

The invention relates to a method for preparing nanometer MgO whiskers at the low temperature and the method is that magnesium powders and amorphous boron powders are mixed according to atomic ratio of MG:B being equal to 1 to 1.5:2 and the mixture is grinded for 30 to 120 minutes for thorough mixing, and after the mixed powders are made into a lump sinter under the pressure of 5 to 10 kg/cm<3> by a press machine, the lump sinter is put into a crucible which is put into a heating zone of an evacuated tubular furnace. The evacuated tubular furnace is sealed, vacuumized to 1 to 10 Pa and filled with argon the oxygen content of which is 2 percent to 5 percent and the flow rate of the mixed gas is 5 to 20 lit. per minute to heat the sample up to 650 to 750 DEG C at the heating rate of 5 to 20 K per minute, and the sample is decreased to the room temperature at the same heating rate after the temperature is kept for 0 to 120 minutes. The surface of the sample forms nanometer MgO whiskers with various appearances and sizes. When reaching 650 DEG C, magnesium evaporates and reacts with the little filled oxygen to produce MgO vapour, and under the lower over-saturation state, MgO whiskers are deposited on a substrate. The method for preparing MgO whiskers needs temperature much lower than the previous and greatly increases the practicality of preparing MgO whiskers.
Owner:TIANJIN UNIV

Corrosion device and method for artificial quartz crystal seed chip

The invention provides a corrosion device for an artificial quartz crystal seed chip. The corrosion device comprises a seed chip main body stander, a corrosion tank and a water-bath tank, wherein a timer and a rotating shaft with a motor are arranged on the seed chip main body stander, the timer is connected with the rotating shaft, and a traction rod is fixedly arranged on the rotating shaft; a rotating wheel capable of freely rotating is arranged on the traction rod, a traction line is fixedly arranged on the rotating wheel, a traction through hole and a venting pipe hole are formed in the top of the corrosion tank, the corrosion tank is placed in a water bath tank, and the traction line sequentially penetrates through a limiting hole and the traction through hole and is fixedly connected with a lifting rope. The invention further discloses a corrosion method for the artificial quartz crystal seed chip. The artificial quartz crystal seed chip can do a reciprocating motion in corrosion liquid. Temperature control of the corrosion liquid is emphasized, the supersaturation degree of the corrosion liquid is effectively controlled, and the uniform-speed corrosion is guaranteed by virtue of the concentration of the corrosion liquid.
Owner:山东博达光电有限公司

Method for in-situ growth of potassium dihydrogen phosphate single crystal in environmental scanning electronic microscope

The invention relates to a method for in-situ growth of potassium dihydrogen phosphate (KDP) single crystal in an environmental scanning electronic microscope (ESEM), belonging to the field of material discipline. The invention applies controllable vacuum environment and temperature changing condition of the ESEM and in-situ grows KDP single crystal and simultaneously in-situ observes the process of dissolving and growing of the KDP. The method prepares the KDP single crystal by the KDP polycrystal powder through controlling water-vapor pressure, relative moisture and the temperature of a sample platform in an ESEM sample chamber; the pressure for dissolving the KDP polycrystal powder is 600 to 670Pa, the temperature is minus 1 to 1 DEG C, and Phi is approximately equal to 100 percent; the pressure for growing the KDP single crystal is 600 to 650Pa, the temperature is 1 to 2.2 DEG C, and Phi is approximately equal to 91 percent to 95 percent. The method is also applicable to grow other water-soluble crystals, and provides methods and conditions for basic problems of dynamically studying microcosmic appearance characteristics and growth mechanism of the water-soluble crystals and the influence of moisture environment to the water-soluble crystals and the like.
Owner:BEIJING UNIV OF TECH

Method for preparing nano catalytic composite materials by utilizing integrating process of ultrasonic-film-anti-solvent method

The invention relates to a method for preparing nano catalytic composite materials by utilizing an integrating process of an ultrasonic-film-anti-solvent method, comprising the following steps of: (1) the ammonium porchlorate saturated solution preparation process: dissolving ammonium porchlorate into a proper solvent to prepare the ammonium porchlorate saturated solution at certain temperature; (2) the dispersing process of a nano catalyst: uniformly dispersing the nano catalyst into an anti-solvent under ultrasonic action; (3) the preparing process: adding the AP (ammonium porchlorate) saturated solution to a nonsolvent through a film tube under certain pressure, wherein after the anti-solvent carries out desolvation on the solvent, the ammonium porchlorate is separated out and covers on the surfaces of uniformly-dispersed nano particles to form the nano catalytic composite materials; (4) filtering and drying processes: firstly carrying out solid-liquid separation on nano composite particles; and (5) the drying process: drying separated materials at 50-150 DEG C to obtain the nano catalytic composite materials. The nano catalytic composite materials prepared by the method have stable structure, uniform nano catalyst dispersion and controllable particle diameter and appearance.
Owner:NANJING NORMAL UNIVERSITY

New technology of applying double-effect forced circulation concentration method in production of ammonium phosphate

The invention provides a new technology of applying the double-effect forced circulation concentration method in the production of ammonium phosphate, which comprises the steps of carrying out double-effect forced circulation flash distillation on phosphoric acid slurry, removing excess moisture in the phosphoric acid slurry and reacting with neutralizing slurry so as to generate intermediate slurry, enabling the intermediate slurry to be reacted with ammonia gas to generate a product, carrying out one-effect forced circulation flash distillation on the product slurry, further preparing qualified monoammonium phosphate slurry, drying and granulating by a fluid bed, packaging and weighing. Heat quantity generated by neutralization reaction is taken as a one-effect flash distillation heat source, and the excess heat in the one-effect flash distillation process is taken as a double-effect flash distillation heat source. With the adoption of the new technology, the heating steps in the production process are reduced, the quantity and height of devices used are decreased, heat energy is used reasonably, and energy consumption is reduced. The temperature difference between an inlet and an outlet of a heater is only 1-3 DEG C, degree of supersaturation can be controlled effectively, and scaling of the pipe wall of a heat exchanger is reduced. The forced circulation can enable the circulation speed of liquid phase to improve greatly, wash the wall pipe, and play an important role in reducing the scaling. The cycle of operation of a device is increased greatly, productive capacity is improved obviously, and the production cost is reduced effectively.
Owner:GANSU WENGFU CHEM

Low-temperature method for manufacturing nano-MgO crystal whisker

The invention relates to a method for preparing nanometer MgO whiskers at the low temperature and the method is that magnesium powders and amorphous boron powders are mixed according to atomic ratio of MG:B being equal to 1 to 1.5:2 and the mixture is grinded for 30 to 120 minutes for thorough mixing, and after the mixed powders are made into a lump sinter under the pressure of 5 to 10 kg / cm<3> bya press machine, the lump sinter is put into a crucible which is put into a heating zone of an evacuated tubular furnace. The evacuated tubular furnace is sealed, vacuumized to 1 to 10 Pa and filledwith argon the oxygen content of which is 2 percent to 5 percent and the flow rate of the mixed gas is 5 to 20 lit. per minute to heat the sample up to 650 to 750 DEG C at the heating rate of 5 to 20K per minute, and the sample is decreased to the room temperature at the same heating rate after the temperature is kept for 0 to 120 minutes. The surface of the sample forms nanometer MgO whiskers with various appearances and sizes. When reaching 650 DEG C, magnesium evaporates and reacts with the little filled oxygen to produce MgO vapour, and under the lower over-saturation state, MgO whiskersare deposited on a substrate. The method for preparing MgO whiskers needs temperature much lower than the previous and greatly increases the practicality of preparing MgO whiskers.
Owner:TIANJIN UNIV

Etching device and etching method of artificial quartz crystal seed wafer

The invention provides a corrosion device for an artificial quartz crystal seed chip. The corrosion device comprises a seed chip main body stander, a corrosion tank and a water-bath tank, wherein a timer and a rotating shaft with a motor are arranged on the seed chip main body stander, the timer is connected with the rotating shaft, and a traction rod is fixedly arranged on the rotating shaft; a rotating wheel capable of freely rotating is arranged on the traction rod, a traction line is fixedly arranged on the rotating wheel, a traction through hole and a venting pipe hole are formed in the top of the corrosion tank, the corrosion tank is placed in a water bath tank, and the traction line sequentially penetrates through a limiting hole and the traction through hole and is fixedly connected with a lifting rope. The invention further discloses a corrosion method for the artificial quartz crystal seed chip. The artificial quartz crystal seed chip can do a reciprocating motion in corrosion liquid. Temperature control of the corrosion liquid is emphasized, the supersaturation degree of the corrosion liquid is effectively controlled, and the uniform-speed corrosion is guaranteed by virtue of the concentration of the corrosion liquid.
Owner:山东博达光电有限公司

A preparation process and device system for continuous cooling and recrystallization of ethyl carbazole

The invention discloses a preparation process and device system for continuous cooling and crystallization of ethyl carbazole, which solves the problem that floating crystals are prone to appear in the process of preparing ethyl carbazole in the traditional process, resulting in high moisture content of crystals and easy preparation of powdery crystals. question. The invention includes a preparation process of continuous cooling and recrystallization of ethyl carbazole. The ethyl carbazole crude product and ethanol solvent are mixed according to the mass ratio, and after heating and dissolving, the temperature is lowered for the first time, and the solution temperature is reduced to a supercooling degree of 1 ℃~4℃, add ethyl carbazole seed crystals with a particle size of 0.05mm~0.1mm, keep warm, and then lower the temperature to the crystallization temperature for the second time to obtain the mother liquor of continuous crystallization. Ultrasonic treatment is carried out on the pre-configured raw material solution, and the crystallization time is controlled, followed by centrifugation, washing and drying to obtain ethyl carbazole granule products; the above-mentioned preparation process is used to provide the device system. The invention has the advantages of being able to continuously cool and recrystallize to prepare short rod-shaped ethyl carbazole, and at the same time completely avoid the generation of floating crystals.
Owner:CHENGDU CHENGDE CHEM TECH

Surface erosion-resistant composite coating of carbon/carbon composite, preparation method and application thereof

The invention relates to a surface erosion-resistant composite coating of a carbon / carbon composite, which sequentially consists of ZrC0.7 / ZrC1.0 / ZrC1.0+C form outside to inside. The preparation method of the surface erosion-resistant composite coating comprises the following three steps: the preparation of a basal layer ZrC1.0+C, the preparation of a middle layer ZrC1.0 and the preparation of anouter-coating layer ZrC0.7; and is characterized in that in a chemical vapor deposition furnace at normal pressure, zirconium tetrachloride is used as the zirconium source, Ar gas is used as the carrier gas, C3H6, acetylene and methane are respectively used as the carbon source gasses, Ar is used as the diluent, H2 is used as the reducing gas, and the surface erosion-resistant composite coating is obtained by deposition at the temperature of 1100-1300 DEG C. The invention has the advantages of simple process method, convenient operation, single heat, stepwise deposition preparation of the composite coating with gradient-changed carbon contents, firm combination between the coating and the basal body, no penetration crack and interlayer crack, and good coating erosion resistance and thermal shock resistance, can realize the industrialized production, and is applicable to the preparation of the erosion-resistant composite coating of the carbon / carbon composite by the chemical gas-phase permeation or the liquid-phase impregnation process.
Owner:CENT SOUTH UNIV

A method for extracting rare earth from ion adsorption type rare earth ore

The invention discloses a method for extracting rare earth from ion adsorption type rare earth ores. The method comprises the following steps: leaching the ion adsorption type rare earth ores by a leaching agent to obtain rare earth leachate; then adding a calcium-alkali compound in the rare earth leachate to remove impurities; adding at least one of magnesium chloride, sodium chloride and potassium chloride in impurity removal mother liquor; and controlling the chloride ion concentration, the temperature and the pH in a precipitation process of the calcium-alkali compound to achieve the purpose of increasing solubility of calcium sulfate and reduce generation of the calcium sulfate in the precipitation process. Meanwhile, under the related conditions of high salinity and the like, the migration speeds of rare earth ions and hydroxyl ions in a precipitation system of the calcium-alkali compound are reduced, the degree of supersaturation of rare earth hydrate is controlled effectively, and crystal precipitates of the rare earth hydrate is facilitated. By the method, ammonia nitrogen pollution is eliminated, formation of the calcium sulfate in the precipitation process of the calcium-alkali compound is reduced, the production cost is reduced, and meanwhile, the product with qualified purity is obtained.
Owner:JIANGXI UNIV OF SCI & TECH

A method for recovering rare earth and aluminum from ion adsorption type rare earth ore

The invention discloses a method for recycling rare earth and aluminum from ion adsorption type rare earth ores. The method comprises the following steps: leaching the ion adsorption type rare earth ores by a leaching agent to obtain rare earth leachate; then adding at least one of magnesium chloride, sodium chloride and potassium chloride in the leachate; and controlling the chloride ion concentration, the temperature and the pH in a precipitation process of a calcium-alkali compound to achieve the purpose of increasing solubility of calcium sulfate and reduce generation of the calcium sulfate in the precipitation process. Meanwhile, under the related conditions of high salinity and the like, the migration speeds of rare earth ions and hydroxyl ions in a precipitation system of calcium oxide are reduced, the degree of supersaturation of rare earth hydrate is controlled effectively, and crystal precipitates of the rare earth hydrate is facilitated. By the method, ammonia nitrogen pollution is eliminated, the rare earth recycling rate is increased, and aluminum resources are recycled comprehensively. Meanwhile, formation of calcium sulfate in the precipitation process of the calcium oxide is reduced, the production cost is reduced, and meanwhile, the product with the qualified purity is obtained. An impurity removal process does not exist in the method, and therefore, loss of rare earth in the impurity removal process can be avoided.
Owner:JIANGXI UNIV OF SCI & TECH

A kind of crystallization method of vitamin C sodium

The invention discloses a crystallization method of sodium ascorbate. A high-purity and large-granularity sodium ascorbate crystal product is prepared by a cooling crystallization and dilution crystallization coupling method through regulation and control of crystallization conditions. The method comprises the following specific technical steps: adding vitamin C and sodium bicarbonate into water; heating to 50 to 60 DEG C to carry out a neutralization reaction; filtering reaction completion liquid through an organic filter membrane, and adding a sodium ascorbate seed crystal; growing the crystal for 1 to 1.5 hours; lowering the temperature by 20 to 30 DEG C to perform first-stage cooling crystallization; raising the temperature by 20 to 30 DEG C, and adding methanol to perform first-stage heating dilution crystallization; performing second-stage cooling crystallization, second-stage heating dilution crystallization and third-stage cooling crystallization; performing centrifugal separation; washing a sodium ascorbate crystal filter cake; performing vacuum drying to obtain a sodium ascorbate crystal product. The crystallization method has high yield, and the obtained sodium ascorbate crystal product has high purity, homogeneous granularity and large crystal main granularity.
Owner:自然资源部天津海水淡化与综合利用研究所

Method for preparing acrylic resin coated nano-drug by solid wall fiber pipe bundle crystallizer

The invention provides a method for preparing an acrylic resin coated nano-drug by a solid wall fiber pipe bundle crystallizer and relates to nano-drug preparation. A water bath device, a dissolving drug bottle, two peristaltic pumps, the fiber pipe bundle crystallizer, a vacuum filtration system and a refrigerator are arranged; the dissolving drug bottle is arranged in the water bath device, an inner pipe and an outer pipe are arranged on the fiber pipe bundle crystallizer, the dissolving drug bottle is connected with an inlet of the first peristaltic pump, an outlet of the first peristaltic pump is connected with an inlet of the inner pipe of the fiber pipe bundle crystallizer, an outlet of the inner pipe of the fiber pipe bundle crystallizer is connected with the vacuum filtration system, an outlet of the outer pipe of the fiber pipe bundle crystallizer is connected with an inlet of the second peristaltic pump, an outlet of the second peristaltic pump is connected with an inlet of the outer pipe of the fiber pipe bundle crystallizer, and the inner pipe of the fiber pipe bundle crystallizer is formed by micron size hollow solid wall fiber pipe bundles. The method comprises the steps of preparation of the fiber pipe bundle crystallizer: single bundles of micron size hollow solid wall fiber pipe bundles are cut and put into a sleeve, and the fiber pipe bundle crystallizer is formed; preparation of the nano-drug and coating of acrylic resin; and postprocessing.
Owner:XIAMEN UNIV

A kind of preparation method of fibrous basic magnesium sulfate whisker

The invention relates to the preparation field of chemical industrial materials, and particularly relates to a preparation method of a fibrous alkali magnesium sulfate whisker. The preparation method of the fibrous alkali magnesium sulfate whisker comprises the following steps: (1) preparing a magnesium sulfate solution by using MgSO4.7H2O, stirring and adding NaOH granular caustic soda, aging for 2-24 hours at the temperature of 25 to 100 DEG C to obtain a slurry; (2) transferring the slurry obtained in the step (1) into a hydrothermal reactor, wherein the filling degree is 50-80 percent, adding 0.5-5 percent of seed crystal according to the mass of the NaOH granular caustic soda, uniformly stirring, and reacting the slurry for 2-12 hours at the temperature of 130-180 DEG C; (3) cooling after finishing the reaction of the step (2), filtering, washing and drying a obtained white turbid liquid to obtain the fibrous alkali magnesium sulfate whisker. According to the preparation method, the seed crystal is added into the reaction slurry, alkali magnesium sulfate is easily subjected to nucleus formation growth, and the preparation concentration of the reaction slurry can be relatively high; the whisker nucleation time is reduced, and the whisker growth time also can be shortened.
Owner:QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI

Crystallization method of sodium ascorbate

The invention discloses a crystallization method of sodium ascorbate. A high-purity and large-granularity sodium ascorbate crystal product is prepared by a cooling crystallization and dilution crystallization coupling method through regulation and control of crystallization conditions. The method comprises the following specific technical steps: adding vitamin C and sodium bicarbonate into water; heating to 50 to 60 DEG C to carry out a neutralization reaction; filtering reaction completion liquid through an organic filter membrane, and adding a sodium ascorbate seed crystal; growing the crystal for 1 to 1.5 hours; lowering the temperature by 20 to 30 DEG C to perform first-stage cooling crystallization; raising the temperature by 20 to 30 DEG C, and adding methanol to perform first-stage heating dilution crystallization; performing second-stage cooling crystallization, second-stage heating dilution crystallization and third-stage cooling crystallization; performing centrifugal separation; washing a sodium ascorbate crystal filter cake; performing vacuum drying to obtain a sodium ascorbate crystal product. The crystallization method has high yield, and the obtained sodium ascorbate crystal product has high purity, homogeneous granularity and large crystal main granularity.
Owner:自然资源部天津海水淡化与综合利用研究所
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